CN102021628A - Method for preparing metal titanium or titanium alloy super-oleophobic surface - Google Patents
Method for preparing metal titanium or titanium alloy super-oleophobic surface Download PDFInfo
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Abstract
The invention discloses a method for preparing a metal titanium or titanium alloy super-oleophobic surface. The method comprises the following steps of: performing primary anodic oxidation treatment on metal titanium or titanium alloy to obtain a roughened surface with a microstructure; forming a titanium dioxide nanotube array film on the surface with microstructure through secondary anodic oxidation so as to obtain a composite fine structured micro-nanostructure; and modifying with a low-surface-energy substance to obtain the super-oleophobic surface and the super-hydrophobic and super-oleophobic surface. The metal titanium or titanium alloy surface has super-oleophobic and super-hydrophobic characteristics for multiple kinds of organic liquid, the static contact angle is greater than 155 degrees; the rolling angle is less than 10 degrees; meanwhile, the surface also shows superior super-oleophobic and super-hydrophobic characteristics for pure water and aqueous solution of acid, alkali and salt.
Description
Technical field
The present invention relates to the preparation method of a kind of metal titanium or the super oleophobic surface of titanium alloy.
Background technology
Wettability is a critical nature of solid surface, is directly determining the performance and the range of application of material.Wettability is mainly by the chemical ingredients of forming solid surface and microtexture decision.In recent years, as a kind of ultimate wettability form, super-hydrophobicity obtains deep research, and many bio-imitability super hydrophobic materials are by the preparing of success, and has obtained Preliminary Applications in automatically cleaning, field such as anticorrosive, antifog.Simultaneously, oleophobic material, particularly super oleophobic material also receives much attention, and how to prepare the focus that super oleophobic surface also day by day becomes people's research.Compare with super hydrophobic material, super oleophobic material still all will have more important role in daily life in industrial production, and this is because oily liquid is easier to bring pollution, and oiliness is polluted also more difficult removal; Equally, if adopt super oleophobic material also will reduce the resistance of petroleum pipe line wall greatly in the petroleum pipe line in the transportation of crude oil, improve conveying efficiency.Yet super oleophobic surface is higher to the requirement of material microstructure, and required modifier surface energy also should be lower, and common super hydrophobic surface can not be realized super oleophobic.Therefore, be the accidental report of in the laboratory, realizing about the super oleophobic of exotic materials in recent years, also there is not correlation engineering application class material to realize super oleophobic.But at micron and nanometer composite structure finishing low surface energy material still is one of the important means of the super oleophobic material of preparation.This type of bibliographical information has: Jiang etc. are with the carbon nano-tube modified array of perfluor siloxanes, super-double-hydrophobic surface (Lei jiang et al, Super-Amphiphobic Aligned Carbon Nanotube Films, Angew.Chem.Int.Ed.2001 have been obtained, 40,1743-1746); People such as Gribaldi adopt the method for electrochemical deposition Polythiophene to obtain stable super-hydrophobic super oleophobic polythiophene film (Serge Gribaldi et al by controlling sedimental pattern and chemical constitution, Synthesis of Stable Super Water-and Oil-Repellent Polythiophene Films, Angew.Chem.Int.Ed.2006,45,2251-2254); People such as Steele utilize the method for spraying ZnO and polymkeric substance to make up coarse structure and have realized super thin (Adam Steele et al to some oils liquid, Inherently Superoleophobic Nanocomposite Coatings by Spray Atomization, Nano Letters, 2009,9,501-505); Application number is 200710303779.4 to disclose underwater ultra-oleophobic polyalcohol membrane of a kind of biomimetic features and preparation method thereof, its method with fish scale as natural template, carry out figuration one time by polydimethylsiloxane, obtain having the template of the negative structure of fish scale, monomer solution in-situ polymerization with polymkeric substance carries out the secondary figuration again, obtains having the underwater ultra-oleophobic polyalcohol membrane of fish scale structure.From this type of document and patent as can be seen, the present general complicated process of preparation of resulting super oleophobic material, materials used is special, narrow application range, and it is narrower to the super thin scope of oily liquid, roll angle is big or fail to provide roll angle, and this has hindered the application of super oleophobic surface in daily productive life greatly.
Titanium and alloy thereof are described as " following metal " as important project class material, are widely used in fields such as aviation and navigation, biomedicine, chemical, are the important new engineering material that tool has great prospects for development.Aspect aerospace, some aircraft with the titanium amount in addition to account for more than 90% of its structure gross weight; Titanium and alloy thereof are applied to the navigation production by wide model again because of its excellent erosion resistance simultaneously.Yet these titanium materials in use inevitably can run into and pollute or corrosion, and particularly the pollution of oily liquid or oil-water mixture and corrosion cause unnecessary loss.Can avoid or alleviate above problem greatly by constructing super-double-hydrophobic surface.Yet it is very difficult to construct super oleophobic surface at engineering materials titanium and alloy surface thereof, does not still have relevant patent or reported in literature so far.Therefore, the exploitation of titanium or titanium alloy surface is a kind of can be super-hydrophobic, the method that particularly can surpass oleophobic just seems particularly important.
Summary of the invention
The object of the present invention is to provide a kind of method at the super oleophobic surface of metal titanium or titanium alloy surface preparation, this surface not only has super oleophobic property, and has the super-double-thinning property of super-hydrophobic, super acidophobic, super thin alkali simultaneously.
The super oleophobic surface of titanium base of the present invention is made up of the chemical modifier of micron and nanometer composite structure that forms in the titanium-based surface anodic oxidation and low surface energy.
The present invention carries out the surface that anodic oxidation treatment obtains the micrometer structure roughening with metal titanium or titanium alloy, and then pass through anodic oxidation for the second time at micrometer structure surface formation layer of titanium dioxide film of Nano tube array, thereby obtain the fine structure of micron and nanometer composite structureization, the modification through the low surface energy material obtains super oleophobic and super-double-hydrophobic surface then.
The preparation method of a kind of metal titanium or the super oleophobic surface of titanium alloy is characterized in that this method steps is as follows:
A is an anode with metal titanium or the titanium alloy after cleaning, and is negative electrode with the graphite flake, carries out the anodic oxidation first time in electrolytic solution, and oxidation current is 0.1-1A/cm
2, oxidization time is 0.5-2h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening; The solute of described electrolytic solution is selected from Na
2SO
4Or NaOH, solvent is selected from distilled water or ethylene glycol;
B carries out the anodic oxidation second time with the titanium or the titanium alloy of micrometer structure roughening in the steps A in electrolytic solution, oxidation voltage is 10-100V, oxidization time is 10min-2h, temperature is 0-25 ℃, form one deck titania nanotube array at titanium or titanium alloy surface, obtain the titanium or the titanium alloy surface of micro nano structureization; The solute of described electrolytic solution is selected from a kind of in hydrochloric acid or the hydrofluoric acid, and solvent is selected from one or both in water, ethylene glycol, glycerol, dimethyl sulfoxide (DMSO) and the methane amide;
C utilizes spin coating or CVD (Chemical Vapor Deposition) method, and perfluor silane or perfluor siloxanes chemistry are modified titanium or the titanium alloy surface that step B obtains, and at 60-120 ℃ of thermal treatment 0.5-2 hour, obtains the super oleophobic property of titanium base surface.
In the A step, the concentration of electrolyte that anodic oxidation is for the first time adopted is 0.5-5wt%.
In the B step, the concentration of electrolyte that anodic oxidation is for the second time adopted is 0.1-5wt%.
Titanium of the present invention or titanium alloy form the micron roughened textures through an anodic oxidation on the surface, form the layer of even nano tube structure through two-step anodization on the micrometer structure surface, the diameter thickness of its nanotube etc. can be controlled by regulating experiment condition, the used low surface energy modifier of last chemically modified is perfluor silane or perfluor siloxanes, this type of modifier combines by forming firm chemical bond with titanium or titanium alloy surface, has very excellent stability.
Titanium or titanium alloy surface that organic liquids such as edible oil, glycerine, methyl iodide and n-Hexadecane are dripped to after chemically modified carry out contact angle determination, and contact angle is all greater than 155 °.Titanium and alloy surface thereof that pure water and soda acid salt brine solution are dripped to after chemically modified carry out contact angle determination, and contact angle is all greater than 160 °.Soaked one month in above-mentioned detection liquid, sample surfaces does not have destroyed, still keeps its super two thin characteristics.
There are the potential purposes in many aspects in titanium of the present invention or titanium alloy surface: titanium base or titanium alloy surface cannot not have stickingly oil, sticking water and the feature of glactaric acid alkali salt not, can be used for the antifouling and antirust of Ti product surface in titanium in the daily living article or titanium alloy vessel or the industrial production; Super oleophobic titanium base or titanium alloy are used for the pipeline material of oil transportation, can realize the conveying of free of losses liquid, and improve transfer rate; Super oleophobic titanium base or titanium alloy are used for all kinds of boats and ships of marine equipment or underwater submarine, can alleviate biological pollution greatly, and are expected to reduce the resistance of water, improve travel speed; Be used for aviation, can reduce atmospheric drag and improve flight velocity, and can reduce the corrosion of corrosive goods confrontation aircraft surfaces materials such as acid rain greatly.
The present invention has the following advantages:
1, preparation technology is simply ripe, and required equipment is simple and easy, and raw material is easy to get.With titanium or titanium alloy is raw material, through two step anodic oxidation and chemically modifieds, prepares super oleophobic surface.
2. because treating processes is carried out in solution,, require lowlyer, can satisfy the demand of various situations so titanium or titanium alloy shape and size are not almost had special requirement.
3, titanium or titanium alloy surface are the micron and nanometer composite structure of micron order structure and nanoscale structures coexistence, the surperficial uniformity of processing, and each place on surface shows the super oleophobic property of indifference and super two thin characteristics.
4, metal titanium or titanium alloy surface have good heat-resisting high-temperature stability and stability, its surface shows as the character of super oleophobic, the super acidophobic alkali salt aqueous solution after chemically modified, promptly to the contact angle of all kinds of organic liquids and the aqueous solution all greater than 150 °, roll angle is less than 10 °.
Embodiment
Embodiment 1
1, being anode to clean the back metal titanium, is negative electrode with the graphite flake, with the Na of metal titanium at 0.1wt%
2SO
4Carry out an anodic oxidation in the aqueous solution, oxidation current is 0.1A/cm
2, oxidization time is 2h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening;
2, the titanium with the micrometer structure roughening is an anode, with the graphite flake is negative electrode, the HCl aqueous solution with 0.1wt% is that electrolytic solution carries out two-step anodization, oxidation voltage is 10V, oxidization time is 2 hours, temperature is 0-5 ℃, forms the layer of even titania nanotube array on micron titanium surface, obtains the titanium surface of micro nano structureization;
3, chemically modified is carried out on the titanium surface that perfluor octadecyl trichlorosilane is spun to micro nano structureization, and at 120 ℃ of thermal treatment 0.5h, can obtain the super oleophobic surface of titanium base.
Experiment titanium-based surface scanning electronic microscope shows that its surface tissue is the compound microtexture of micron projection with nanotube; N-Hexadecane and rapeseed oil are 155 ° and 160 ° at this lip-deep static contact angle, and roll angle is less than 10 °; Pure water and soda acid salt brine solution static contact angle are all greater than 160 °.
Embodiment 2
1, being anode to clean the back metal titanium, is negative electrode with the graphite flake, and metal titanium is carried out an anodic oxidation in the NaOH of the 5wt% aqueous solution, and oxidation current is 0.5A/cm
2, oxidization time is 1h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening;
2, the titanium with the micrometer structure roughening is an anode, with the graphite flake is negative electrode, HCl ethylene glycol solution with 5wt% is that electrolytic solution carries out two-step anodization, oxidation voltage is 100V, oxidization time is 10min, temperature is 10 ℃, forms the layer of even titania nanotube array on micron titanium surface, obtains the titanium surface of micro nano structureization;
3, chemically modified is carried out on the titanium surface that perfluor octadecyl trichlorosilane is spun to the good micro nano structureization of drying, and at 100 ℃ of thermal treatment 1h, can obtain the super oleophobic surface of titanium base.
Experiment titanium-based surface scanning electronic microscope shows that its surface tissue is the compound microtexture of micron projection with nanotube; N-Hexadecane and ionic liquid are 156 ° and 162 ° at this lip-deep static contact angle, and roll angle is less than 10; Pure water and soda acid salt brine solution static contact angle are all greater than 160 °.
Embodiment 3
1, being anode to clean the back titanium alloy, is negative electrode with the graphite flake, with the Na of metal titanium at 5wt%
2SO
4Carry out an anodic oxidation in the ethylene glycol solution, oxidation current is 1A/cm
2, oxidization time is 0.5h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening;
2, the titanium with surperficial micrometer structure roughening is an anode, with the graphite flake is negative electrode, HF formamide soln with 0.1wt% is that electrolytic solution carries out two-step anodization, oxidation voltage is 20V, oxidization time is 30min, temperature is 0 ℃, forms the layer of even titania nanotube array on micron titanium surface, obtains the titanium surface of micro nano structureization;
3, utilize the method for vapour deposition that the perfluoro capryl silicone deposition is carried out chemically modified to the titanium surface of the good micro nano structureization of drying, and, can obtain the super oleophobic surface of titanium base at 80 ℃ of thermal treatment 1.5h.
Experiment titanium-based surface scanning electronic microscope shows that its surface tissue is the compound microtexture of micron projection with nanotube; N-Hexadecane and glycerine are 156 ° and 165 ° at this lip-deep static contact angle, and roll angle is less than 10 °; Pure water and soda acid salt brine solution static contact angle are all greater than 160 °.
Embodiment 4
1, being anode to clean the back titanium alloy, is negative electrode with the graphite flake, and metal titanium is carried out an anodic oxidation in the NaOH of 0.1wt% ethylene glycol solution, and oxidation current is 0.5A/cm
2, oxidization time is 1h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening;
2, the titanium with surperficial micrometer structure roughening is an anode, with the graphite flake is negative electrode, HF dimethyl sulphoxide solution with 5wt% is that electrolytic solution carries out two-step anodization, oxidation voltage is 50V, oxidization time is 1h, temperature is a room temperature, forms the layer of even titania nanotube array on micron titanium surface, obtains the titanium surface of micro nano structureization;
3, utilize the method for vapour deposition that the perfluoro capryl silicone deposition is carried out chemically modified to the titanium surface of micro nano structureization, and, can obtain the super oleophobic surface of titanium base at 60 ℃ of thermal treatment 2h.
Experiment titanium-based surface scanning electronic microscope shows that its surface tissue is the compound microtexture of micron projection with nanotube; N-Hexadecane and methyl iodide are 155 ° and 170 ° at this lip-deep static contact angle, and roll angle is less than 10 °; Pure water and soda acid salt brine solution static contact angle are all greater than 160 °.
Claims (3)
1. the preparation method of metal titanium or the super oleophobic surface of titanium alloy is characterized in that this method steps is as follows:
A is an anode with metal titanium or the titanium alloy after cleaning, and is negative electrode with the graphite flake, carries out the anodic oxidation first time in electrolytic solution, and oxidation current is 0.1-1A/cm
2, oxidization time is 0.5-2h, reaction finishes the back ultrasonic cleaning and removes oxide compound and supernatant liquid, obtains the titanium-based surface of micrometer structure roughening; The solute of described electrolytic solution is selected from Na
2SO
4Or NaOH, solvent is selected from distilled water or ethylene glycol;
B carries out the anodic oxidation second time with the titanium or the titanium alloy of micrometer structure roughening in the steps A in electrolytic solution, oxidation voltage is 10-100V, oxidization time is 10min-2h, temperature is 0-25 ℃, form one deck titania nanotube array at titanium or titanium alloy surface, obtain the titanium or the titanium alloy surface of micro nano structureization; The solute of described electrolytic solution is selected from a kind of in hydrochloric acid or the hydrofluoric acid, and solvent is selected from one or both in water, ethylene glycol, glycerol, dimethyl sulfoxide (DMSO) and the methane amide;
C utilizes spin coating or CVD (Chemical Vapor Deposition) method, and perfluor silane or perfluor siloxanes chemistry are modified titanium or the titanium alloy surface that step B obtains, and at 60-120 ℃ of thermal treatment 0.5-2 hour, obtains the super oleophobic property of titanium base surface.
2. the method for claim 1 is characterized in that: in the A step, the concentration of electrolyte that anodic oxidation is for the first time adopted is 0.5-5wt%.
3. the method for claim 1 is characterized in that: in the B step, the concentration of electrolyte that anodic oxidation is for the second time adopted is 0.1-5wt%.
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